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Publication numberUS20060042415 A1
Publication typeApplication
Application numberUS 10/928,203
Publication dateMar 2, 2006
Filing dateAug 30, 2004
Priority dateAug 30, 2004
Also published asUS7291201
Publication number10928203, 928203, US 2006/0042415 A1, US 2006/042415 A1, US 20060042415 A1, US 20060042415A1, US 2006042415 A1, US 2006042415A1, US-A1-20060042415, US-A1-2006042415, US2006/0042415A1, US2006/042415A1, US20060042415 A1, US20060042415A1, US2006042415 A1, US2006042415A1
InventorsJeng-Gong Duh, Li-Yin Hsiao
Original AssigneeJeng-Gong Duh, Li-Yin Hsiao
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Method for making nano-scale lead-free solder
US 20060042415 A1
Abstract
A method for making Nano-scale lead-free solder includes the following steps of: forming a mixture solution Sn—Ag or Sn—Ag—Cu; making NaBH4, NaOH and alkyl C12H25OSO3Na to a reducing dispersing solution; producing reactant Sn—Ag or Sn—Ag—Cu by means of the oxidation reduction method; and adding 95% ethanol to be mixed, and cleaning the reactant by using a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale (0.1˜100 nm) lead-free solder Sn-3.5Ag or Sn-3.5Ag-xCu (x=0.2˜1.0).
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Claims(4)
1. A method for making Nano-scale lead-free solder, the lead-free solder being Sn-3.5Ag (96.5Sn-3.5Ag), comprising the following steps of:
(a) mixing a pre-determined amount SnSO4(aq) and a pre-determined amount AgNO3(aq) to 0.4 liter and then to form a mixture solution Sn—Ag which has a weight ratio of Sn and Ag being 96.5:3.5;
(b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution;
(c) adding the mixture solution Sn—Ag in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn and Ag by means of the oxidation reduction between both solutions; and
(d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale lead-free solder Sn-3.5Ag.
2. The method according to claim 1, wherein the mole number of the reducing agent NaBH4 is 5 times the total mole number of SnSO4(aq) and AgNO3(aq) in the step (a).
3. A method for making Nano-scale lead-free solder, the lead-free solder being Sn-3.5Ag-xCu (x=0.2˜1.0), comprising the following steps of:
(a) mixing a pre-determined amount SnSO4(aq), a pre-determined amount AgNO3(aq) and Cu(NO3)2(aq) to 0.4 liter and then to form a mixture solution Sn—Ag—Cu which has a weight ratio of Sn, Ag and Cu being (96.5−x):3.5:x, wherein x=0.2˜1.0;
(b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution;
(c) adding the mixture solution Sn—Ag—Cu in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn, Ag and Cu by means of the oxidation reduction between both solutions; and
(d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using supersonic vibration of a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale lead-free solder Sn-3.5Ag-xCu, wherein x=0.2˜1.0.
4. The method according to claim 3, wherein the mole number of the reducing agent NaBH4 is 5 times the total mole number of SnSO4(aq) and AgNO3(aq) in the step (a).
Description
FIELD OF THE INVENTION

The present invention relates to a method for making Nano-scale lead-free solder, and more particularly to a method for making Nano-scale (0.1˜100 nm) lead-free solder.

BACKGROUND OF THE INVENTION

A solder of a contact mainly provides electric conductivity and mechanical strength disposed between an electronic component and a circuit board and is a path for spreading heat during operating, and therefore the solder is very important to an electronic product. Conventional tin-lead (Sn—Pb) solder has low cost, good wetting property, proper fusing point, proper electric conductivity, proper mechanical strength and proper thermal conductivity, and therefore tin-lead (Sn—Pb) solder has been widely applied in the field of industry. However, lead (Pb) is a toxic heavy metal, and seriously affects health of human body. Thus, various countries gradually have laws and decrees to restrain or stop using the solder with lead. In 1998, a conference of global same trade organization is held in Wiesbaden, Germany by PCB makers who are from various countries, and is concluded that various countries stop using the solder with lead from 2004. Although the conclusion of stopping using the solder with lead is changed from 2004 to July, 2006 because of some reason, the lead-free solder still become a challenge of electronic industry in the future.

The Nano-scale Electronic Age comes, and the electronic device has tendencies towards minimization, low lightweight and high functional requirement and then the electronic packaging technology has tendencies towards higher I/O density and shorter contact pitch. Thus, the high density connection technologies, such as flip chip connection, chip scale package (CSP) and direct chip attachment (DCA), are main stream of the future electronic packaging technology, but the technology of connection between components is a key technology.

As the minimization of an integrated circuit (IC) and the complexity of a circuit are required, the soldering point of the corresponding electronic component has a tendency towards minimization. Conventional solder is formed by “an electroplate method” or “a silk screen printing method”. However, the above-mentioned methods mostly form micrometer-scale solder (100˜1000 nm), and cannot form a useful Nano-scale (0.1˜100 nm) lead-free solder according to the Nano-scale (0.1˜100 nm) soldering point of the electronic component.

SUMMARY OF THE INVENTION

It is an object of the present invention to provide a method which can improve the size of conventional lead-free solder and make Nano-scale (0.1˜100 nm) lead-free solder. The method is effectively applied to the process of commercial mass production.

It is another object of the present invention to provide a method for making various Nano-scale (0.1˜100 nm) lead-free solder of Sn-3.5Ag and Sn-3.5Ag-xCu (x=0.2˜1.0).

In order to achieve the foregoing objects, the present invention provides a method for making Nano-scale lead-free solder including the following steps of: (a) mixing a pre-determined amount SnSO4 (aq) and a pre-determined amount AgNO3(aq) to 0.4 liter and then to form a mixture solution Sn—Ag which has a weight ratio of Sn and Ag being 96.5:3.5; (b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution; (c) adding the mixture solution Sn—Ag in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn and Ag by means of the oxidation reduction between both solutions; and (d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale lead-free solder Sn-3.5Ag.

The present invention further provides a method for making Nano-scale lead-free solder including the following steps of: (a) mixing a pre-determined amount SnSO4(aq), a pre-determined amount AgNO3(aq) and Cu(NO3)2(aq) to 0.4 liter and then to form a mixture solution Sn—Ag—Cu which has a weight ratio of Sn, Ag and Cu being (96.5−x):3.5:x, wherein x=0.2˜1.0; (b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution; (c) adding the mixture solution Sn—Ag—Cu in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn, Ag and Cu by means of the oxidation reduction between both solutions; and (d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using supersonic vibration of a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale lead-free solder Sn-3.5Ag-xCu, wherein x=0.2˜1.0.

The foregoing, as well as additional objects, features and advantages of the invention will be more readily apparent from the following detailed description, which proceeds with reference to the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a XRD diagram showing the Nano-scale lead-free solder Sn-3.5Ag produced by the present invention.

FIG. 2 is a SEM image showing the lead-free solder Sn-3.5Ag produced by the present invention

FIG. 3 is a XRD diagram showing the Nano-scale lead-free solder Sn-3.5Ag-0.2Cu, Sn-3.5Ag-0.5Cu and Sn-3.5Ag-1.0Cu produced by the present invention.

FIG. 4 is a SEM image showing the lead-free solder Sn-3.5Ag-0.2Cu produced by the present invention.

FIG. 5 is a SEM image showing the lead-free solder Sn-3.5Ag-0.5Cu produced by the present invention.

FIG. 6 is a SEM image showing the lead-free solder Sn-3.5Ag-1.0Cu produced by the present invention.

FIG. 7 is a DSC diagram showing the Nano-scale lead-free solder Sn-3.5Ag and Sn-3.5Ag-0.2Cu produced by the present invention.

DESCRIPTION OF THE PREFERRED EMBODIMENTS

The present invention provides a method for making Nano-scale lead-free solder, and the lead-free solder is Sn-3.5Ag (96.5Sn-3.5Ag), i.e. the weight ratio of Sn to Ag is 96.5:3.5 by means of metal material mixture. The method includes the following steps of:

(a) mixing a pre-determined amount SnSO4(aq) and a pre-determined amount AgNO3(aq) to 0.4 liter and then to form a mixture solution Sn—Ag which has a weight ratio of Sn and Ag being 96.5:3.5;

(b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution, wherein the mole number of the reducing agent NaBH4 is 5 times the total mole number of SnSO4(aq) and AgNO3(aq) in the step (a);

(c) adding the mixture solution Sn—Ag in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn and Ag by means of the oxidation reduction between both solutions; and

(d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using supersonic vibration of a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale (0.1˜100 nm) lead-free solder Sn-3.5Ag.

Referring FIG. 1, it is a XRD diagram showing the Nano-scale lead-free solder Sn-3.5Ag produced by the present invention by utilizing X-ray diffractometer (XRD). As the phase of Ag3Sn is shown in FIG. 1, the Nano-scale lead-free solder Sn-3.5Ag of the present invention is a uniformly mixed lead-free solder Sn-3.5Ag. Referring FIG. 2, it is an SEM image showing the lead-free solder Sn-3.5Ag produced by the present invention by utilizing scanning electron microscopy (SEM).

The present invention provides another method for making Nano-scale lead-free solder, and the lead-free solder Sn-3.5Ag-xCu (x=0.2˜1.0) is also produced by an oxidation reduction method, i.e., the lead-free solder is a metal material mixture which includes Sn, Ag and Cu. The method includes the following steps of:

(a) mixing a pre-determined amount SnSO4(aq), a pre-determined amount AgNO3(aq) and Cu(NO3)2(aq) to 0.4 liter and then to form a mixture solution Sn—Ag—Cu which has a weight ratio of Sn, Ag and Cu being (96.5−x):3.5:x, wherein x=0.2˜1.0;

(b) making a reducing agent NaBH4, 1 M NaOH and 0.01 M alkyl sodium sulfate (C12H25OSO3Na is a dispersing agent) to a liter of reducing dispersing solution, wherein the mole number of the reducing agent NaBH4 is 5 times the total mole number of SnSO4(aq) and AgNO3(aq) in the step (a);

(c) adding the mixture solution Sn—Ag—Cu in the step (a) to the reducing dispersing solution during fast stirring the reducing dispersing solution, thereby producing reactant Sn, Ag and Cu by means of the oxidation reduction between both solutions; and

(d) settling the reactant in the step (c), then adding 95% ethanol to be mixed, and cleaning the reactant by using supersonic vibration of a supersonic vibrator for removing boron (B) and sulfur (S) atom which adhere to the reactant, thereby producing the Nano-scale (0.1˜100 nm) lead-free solder Sn-3.5Ag-xCu (x=0.2˜1.0).

Referring FIG. 3, it is a XRD diagram showing the Nano-scale lead-free solder Sn-3.5Ag-0.2Cu, Sn-3.5Ag-0.5Cu and Sn-3.5Ag-1.0Cu produced by the present invention by utilizing X-ray diffractometer (XRD). As the phase of Ag3Sn and Cu6Sn5 is shown in FIG. 3, the Nano-scale lead-free solder Sn-3.5Ag-xCu (x=0.2˜1.0) of the present invention is a uniformly mixed lead-free solder Sn-3.5Ag-xCu (x=0.2˜1.0). Referring FIGS. 4 to 6, they are SEM images showing the lead-free solder Sn-3.5Ag-0.2Cu, Sn-3.5Ag-0.5Cu and Sn-3.5Ag-1.0Cu produced by the present invention by utilizing scanning electron microscopy (SEM).

Referring FIG. 7, it is a differential scanning calorimetry (DSC) diagram showing the Nano-scale lead-free solder Sn-3.5Ag and Sn-3.5Ag-0.2Cu produced by the present invention. As the measured curves of Sn-3.5Ag and Sn-3.5Ag-0.2Cu are shown in FIG. 7, there is one absorption peak only, such that the Nano-scale (0.1˜100 nm) lead-free solder Sn-3.5Ag and Sn-3.5Ag-0.2Cu of the present invention is a uniformly mixed lead-free solder.

The above-mentioned examples only disclose some of the preferred embodiments of the present invention. The condition of method for making the Nano-scale lead-free solder includes the solution having metal ion of Sn, Ag and Cu which all can depend on the metal mixture of the lead-free solder.

Although the invention has been explained in relation to its preferred embodiment, it is not used to limit the invention. It is to be understood that many other possible modifications and variations can be made by those skilled in the art without departing from the spirit and scope of the invention as hereinafter claimed.

Referenced by
Citing PatentFiling datePublication dateApplicantTitle
CN102189270A *May 4, 2011Sep 21, 2011上海大学Method for chemically synthesizing nano lead-free solder particles with low melting point
Classifications
U.S. Classification75/371
International ClassificationB22F9/24
Cooperative ClassificationB82Y30/00, C22C1/04, B22F1/0018, C22C13/00, B23K35/262, B23K35/0244, B22F9/24, B23K35/34
European ClassificationB82Y30/00, C22C13/00, B22F1/00A2B4, B23K35/26B, C22C1/04, B22F9/24
Legal Events
DateCodeEventDescription
Aug 30, 2004ASAssignment
Owner name: NATIONAL TSING HUA UNIVERSITY, CHINA
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:DUH, JENQ-GONG;HSIAO, LI-YIN;REEL/FRAME:015751/0806
Effective date: 20040810
Apr 7, 2011FPAYFee payment
Year of fee payment: 4
Apr 21, 2015FPAYFee payment
Year of fee payment: 8